Process for producing sputtering target materials

ABSTRACT

The invention includes methods of reducing grain sizes of materials, and methods of forming sputtering targets. The invention includes a method for producing a sputtering target material in which a metallic material is subjected to plastic working at a processing percentage of at least 5% and a processing rate of at least 100%/second. In particular applications the metallic material comprises one or more of aluminum, copper and titanium.

RELATED PATENT DATA

[0001] This application claims priority under 35 U.S.C. §119 to JapanesePatent application reference number 92032, which was filed Oct. 15,1999, entitled “Process For Producing Sputtering Target Material”, andwhich lists Lijun Yao as an inventor. This application also claimspriority under 35 U.S.C. §119 to Japanese Patent application referencenumber 02193, which was filed Apr. 28, 2000, entitled “Process ForProducing Sputtering Target Material”, and which lists Lijun Yao as aninventor.

TECHNICAL FIELD

[0002] The present invention relates to a process for producing amaterials with reduced grain sizes, and can be used, for example, toproduce sputtering target materials (i.e., physical vapor depositiontarget materials, and it is to be understood that in the context of thisdocument the terms “physical vapor deposition” and “sputtering” can beused interchangeably). In particular applications, the sputtering targetmaterials can comprise titanium, aluminum or copper. The sputteringtarget materials can hereinafter be referred to as a “target materials”.

BACKGROUND OF THE INVENTION

[0003] The quality of a thin film formed on a substrate by a sputteringmethod can be influenced by the surface roughness of a target materialused for the sputtering. When protrusions having a larger size than acertain level are present on the surface of the target material, anabnormal discharge (so-called micro-arcing) can be caused at theprotrusions. The abnormal discharge can result in macroparticles beingscattered out from the surface of the target material, and depositedonto the substrate. The deposited macroparticles can cause blobs on thethin film and result in short circuiting of semiconductor thin filmcircuits. The deposited macroparticles are usually called “particles” or“splats”.

[0004] The surface roughness of a target material can have a correlationto a crystal grain size of the target material. The finer the crystalgrain size, the smaller the surface roughness of the target material.Accordingly, by reducing the size of crystal grains existing within thetarget material, it is possible to prevent the generation of the“particles”, thereby allowing better quality thin films to be formedthan can be formed from targets having larger grain sizes.

[0005] Numerous materials can be utilized as target materials,including, for example, copper, aluminum and titanium. In particularapplications, target materials can comprise alloys or other metallicmixtures, with exemplary mixtures comprising one or more of copper,aluminum or titanium. Target materials can also comprise so-called “highpurity” forms of particular metallic materials, with exemplary targetsbeing from 99.99% pure to greater than 99.9999% pure in one or more oftitanium, aluminum and copper.

[0006] Several methods have been proposed for forming improved targetconstructions.

[0007] In Japanese Patent Application Laid-Open (KOKAI) No. 11-54244(1999), there has been proposed a target material composed of titaniumand having an average crystal grain size of 0.1 to 5 μm. The targetmaterial is produced by hydrogenating titanium, subjecting the titaniumto plastic working while maintaining an α-phase or (α-β)-phase crystalstructure thereof, and then dehydrogenating and heat-treating thetitanium.

[0008] However, a production method which includes hydrogenation anddehydrogenation treatments can be problematic from the industrialviewpoint. Consequently, it would be desirable to develop an alternativeprocess for producing a titanium target material.

[0009] Another method proposed for forming an improved targetconstruction is set forth in Japanese Patent Application Laid-Open(KOKAI) No. 10-330928 (1998). Such proposes a sputtering target materialmade of an aluminum alloy and containing crystal grains having anaverage diameter of not more than 30 μm. The target material is producedby subjecting a raw metal material to plastic working, and then rapidlyheating the metal material to a re-crystallizable temperature. The rapidheating utilizes an average temperature increase ramp rate of 100°C./minute. A difficulty with the production method of KOKAI No.10-330928 is that it can require a special heating method to accomplishthe rapid heating, with exemplary special heating methods including aninfrared irradiation method, an electromagnetic induction heating methodor an immersion method using either a salt bath or a bath of low-meltingalloy such as solder. Thus, the production method can be difficult toincorporate cost-effectively into industrial processes. Accordingly, itwould be desirable to develop alternative processes for producingaluminum target materials.

SUMMARY OF THE INVENTION

[0010] The invention encompasses methods of reducing grain sizes ofmaterials, and in particular applications encompasses methods ofreducing grain sizes of titanium-comprising materials,aluminum-comprising materials, and/or copper-comprising materials. Theinvention further encompasses methods of forming sputtering targets. Ina particular embodiment, the invention encompasses a method forproducing a sputtering target material in which a metallic material issubjected to plastic working at a processing percentage of at least 5%utilizing a processing rate of at least 100% per second (i.e.,100%/second). In particular applications the metallic material comprisesone or more of aluminum, copper and titanium.

BRIEF DESCRIPTION OF THE DRAWINGS

[0011] Preferred embodiments of the invention are described below withreference to the following accompanying drawings.

[0012]FIG. 1 is a diagrammatic, cross-sectional view of an apparatuswhich can be utilized in a process encompassed by the present invention,and illustrates a raw material in the apparatus at a preliminaryprocessing step.

[0013]FIG. 2 is a view of the FIG. 1 apparatus and shows the material ofFIG. 1 at a processing step subsequent to that of FIG. 1.

[0014]FIG. 3 is a exploded view of the FIG. 1 apparatus and materialafter the processing step of FIG. 2.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0015] The present invention can overcome at least some of the problemsdescribed above in the “BACKGROUND” section of this disclosure.Specifically, the present invention can provide an industrially usefulprocess for producing materials with reduced grain sizes, and can beutilized, for example, to form a sputtering target material thatgenerates few “particles” during film formation. In particular aspects,the invention comprises methods of forming targets which comprise one ormore of aluminum, copper and titanium.

[0016] In one aspect of the invention, it has been found that byappropriately controlling plastic working conditions used for theproduction of a material, specifically a processing rate thereof, it ispossible to reduce the size of crystal grains of the material. Thereduction of crystal grain size can improve sputtering properties of asputtering target formed from the material relative to targets formedfrom materials having larger grain sizes.

[0017] Aspects of the present invention are described in detail below.In particular described aspects, titanium is used as a raw materialwhich is subjected to appropriate processing to reduce a grain sizewithin the material. The titanium materials can include materials formedby melting sponge-like titanium with a vacuum metallurgy method or thelike, and then casting the melt into titanium ingots. In exemplaryembodiments of the present invention, titanium-comprising materials areutilized which comprise high-purity titanium having a purity of 99.99 to99.9999% by weight (4N to 6N), or greater.

[0018] The invention also comprises utilization of copper as a rawmaterial, and in exemplary embodiments copper-comprising materials areutilized which comprise high-purity copper having a purity of 99.99 to99.9999% by weight, or greater. Another aspect of the invention utilizesaluminum, or an alloy thereof, as a raw material, and in exemplaryembodiments aluminum-comprising materials are utilized which comprisehigh-purity aluminum having a purity of 99.99 to 99.9999% by weight, orgreater. The aluminum-comprising materials can further comprise one moreelements in addition to the aluminum, with said one or more elementsincluding at least one element selected from the group consisting of Si,Cu, Ti, Cr, Mn, Zr, Hf and rare earth elements (such as Sc, Y or Nd).The total amount of additional elements added to the aluminum of atarget material is usually from 0.01% to 10% (by weight), and can befrom 0.03% to 3% (by weight).

[0019] A process of the present invention can include plastic working ofa material until a processing percentage of at least 5% is reached. Thematerial can comprise one or more of titanium, aluminum and copper. Theplastic working can be utilized to control the crystal orientationcontent of the processed material. As utilized herein, “plastic working”refers to processing which deforms a raw material. An exemplary plasticworking process is rolling. A deformation percentage (percentage ofreduction in thickness) of the raw material upon such a processing iscalled “processing percentage”. In the present invention, the upperlimit of the processing percentage is typically about 90%. A “processingrate” is a rate at which a material is deformed, and is expressed interms of an amount of compression per unit time. For instance, aprocessing rate of 100%/second means that a material is compressed at arate such that a compressing die would travel an entirety of thematerial's original thickness in one second; a rate of 500%/second meansthat a material is compressed at a rate such that a compressing diewould travel five-times the material's original thickness in one second;etc. In one aspect of the invention, a process for reducing a grain sizeof a metal-comprising raw material comprises subjecting the material toplastic working at a processing percentage of at least 5% whilemaintaining a processing rate of at least 100%/second. In other words,the processing rate utilized to obtain the processing percentage of atleast 5% is at least 100%/second. It is noted that a processing ratewill typically slow during a plastic working process from an initialrapid rate to a rate of zero as the compressing die compresses amaterial and subsequently comes to a rest on the compressed material. Inpreferred embodiments, the processing rate will remain equal to orgreater than 100%/second during at least a 5% compression of a workedmaterial.

[0020] An important feature of the present invention can be that itincludes subjecting a material to plastic working at high processingrates (i.e., at processing rates of at least 100%/second). Processingrates of the present invention can be at least 500%/second, and inparticular embodiments of the invention are at least 1,000%/second. Theupper limit of the processing rate is usually about 10,000%/second. Incontrast to the processing rates of the present invention, theprocessing rates conventionally used for the plastic working are lowprocessing rates of less than 100%/second, such as, for example, about20%/second. Thus, the present invention utilizes a higher processingrate than conventional methods.

[0021] An apparatus 10 which can be utilized in methodology of thepresent invention is described with reference to FIGS. 1-3. Referring toFIG. 1, apparatus 10 comprises a support 12 having a first die 14thereon. A material 16 is provided on first die 14 for processing.Material 16 can comprise, for example, a high purity titanium, copper oraluminum ingot. A second die 18 is provided above material 16, andconfigured to mate within first die 14. First die 14 can define a shapethat material 16 is too be pressed into, such as, for example, a roundsputtering target shape. A power source (not shown) can be connected tosecond die 18 and utilized to press second die 18 into first die 16 at adesired processing rate. It is noted that the power source can becoupled to one or both of first die 14 and support 12, alternatively to,or in addition to, being coupled with first die 18. It is also notedthat first die 18 can be a heavy “hammer”, formed of, for example, iron,which is elevated above first die 14 and then subsequently dropped ontothe first die. An exemplary hammer has a weight of about 4 tons. Therate of processing applied by such hammer can be controlled bycontrolling the height from which the hammer is dropped.

[0022] Referring to FIG. 2, apparatus 10 is shown after second die 18has compressed material 16 into first die 14.

[0023] Referring to FIG. 3, apparatus 10 and material 16 are shown in anexploded view after the processing of FIG. 2 to illustrate material 16separate from apparatus 10, and to show that material 16 has beencompressed into a shape defined by first die 14.

[0024] The use of the high processing rates of the present invention canprovide several advantages, including that the high processing rates canenable the heat-treatment ordinarily required subsequent to the plasticworking to be omitted. Instead, high processing rates of methods of thepresent invention can allow the plastic working itself to enable crystalgrains of the obtained target material to be well-controlled in size(i.e., become finer).

[0025] The present invention can be particularly useful for processingtitanium.

[0026] Titanium target materials produced by processes according to thepresent invention can have an average titanium crystal grain size of notmore than 4 μm. Titanium-comprising thin films obtained by sputterdeposition from such targets can have reduced amounts of “particles”generated thereon relative to films formed by sputtering fromconventionally produced targets. Exemplary targets produced by methodsof the present invention, and exemplary films sputtered from suchtargets, are described in Examples below.

[0027] The present invention can be also be particularly useful forprocessing aluminum and alloys of aluminum. Aluminum-comprising targetmaterials produced by processes according to the present invention canhave an average crystal grain size of not more than 20 μm.Aluminum-comprising thin films obtained by sputter deposition from suchtargets can have reduced amounts of “particles” generated thereonrelative to films formed by sputtering from conventionally producedtargets. Exemplary targets produced by methods of the present invention,and exemplary films sputtered from such targets, are described inExamples below.

[0028] The above-described high-rate plastic working of the presentinvention is preferably repeated a plurality of times on a givenprocessed material. More specifically, it can be preferred that thehigh-rate plastic working be repeated two or more times. The differentplastic working steps can occur along the same axis dimensions ofmaterial as one another, or along different axis dimensions. It can bepreferred that the different plastic working steps involve at leastthree separate steps, with a first step having pressure applied in afirst axis direction of a material (e.g., an X-axis or Y-axisdirection); a second step having pressure applied in a second axisdirection of the material (the second axis direction can beperpendicular to the first axis direction); and a third step havingpressure applied again along the first axis direction.

[0029] In a particular example, a round rod-shaped raw material is used,and two or more high-rate plastic working processes are conducted tospread the round bar-shaped raw material (e.g., forging). Also, alow-rate plastic working is utilized to elongate the round rod-shapedraw material by applying a pressure thereto in the circumferentialdirection (plastic working similar to swaging). The low-rate plasticworking step is interposed between two of the high-rate plastic workingsteps. The swaging-like plastic working is typically conducted at lowprocessing rates because it can be difficult to conduct suchswaging-like plastic working at high-rate processing.

[0030] The low-rate plastic working and the high-rate plastic workingare usually performed by a hydraulic press method and a hammer pressmethod, respectively. The hammer press method enables the processingrate to be readily controlled by changing a drop height of an ironhammer. The maximum number of repeated high-rate plastic workingprocesses is not particularly restricted, and the high-rate plasticworking is usually repeated three to five times.

[0031] Subjecting a raw material to the above-described high-rateplastic working of the present invention can impart desired propertiesof a sputtering target to the material. The high-rate plastic working ofa material is preferably conducted until a processing percentage of atleast 5% is reached, while the low-rate plastic working can be conductedat an optional processing percentage.

[0032] A raw material can be heated by a spontaneous heat produced uponthe plastic working during high-rate processing of the presentinvention. It can be preferred that a raw material comprising titaniumbe maintained at a temperature of not more than 400° C. during theplastic working. When the temperature of the raw material is more than400° C., the raw material can suffer from abrupt crystal growth, whichcan render it difficult to obtain fine crystal grains. It can also bepreferred that a raw material comprising aluminum (such as, for example,a material comprising either pure aluminum, or an aluminum alloy) bemaintained at a temperature of from about 50° C. to about 450° C. duringthe plastic working. When the temperature of an aluminum-comprising rawmaterial is more than 450° C., the raw material can suffer from abruptcrystal growth, which can render it difficult to obtain fine crystalgrains.

[0033] A titanium-comprising target material produced by a process ofthe present invention can have an average crystal grain size of not morethan 4 μm, and preferably not more than 2 μm. A lower limit of theaverage crystal grain size of a titanium-comprising target material isusually 0.1 μm. In interpreting this disclosure and the claims thatfollow, the term “average grain size” refers to a mean grain size.Targets produced by methodology of the present invention will preferablyhave relatively tight distributions of grains sizes. In particularexamples, the distribution will be such that at least 99% of the grainsof a target will be within a factor of 10 of the mean grain size.

[0034] An aluminum-comprising target material produced by a process ofthe present invention can have an average crystal grain size of not morethan 20 μm, and preferably not more than 10 μm. A lower limit of theaverage crystal grain size of an aluminum-comprising target material isusually 0.1 μm.

EXAMPLES

[0035] The invention is illustrated by, but not limited to, thefollowing examples.

Titanium Processing Examples Examples 1-6 and Comparative Examples 1-5(Shown in Table 2)

[0036] A round, rod-shaped titanium ingot having a diameter of 150 mm, alength of 150 mm and a purity of 99.995% (by weight) is subjected to theplastic working steps (a) through (d) that are described below inTable 1. The plastic working steps were continuously conducted threetimes. Subsequent to the plastic working, a further plastic working forspreading the raw material (forging) was conducted at a processing rateof 20%/second, thereby forming the raw material into an appropriateshape and obtaining a target material having a size of 410 mm indiameter ×20 mm in length. TABLE 1 Final Dimension Pressure-applyingProcessing Processing (diameter direction Percentage Rate mm ×(phenomenon) (%) (%/sec.) length) (a) Circumferential 8.7 20 137 × 180direction (elongation) (b) Axial direction 44.4 Speed described in 184 ×100 (spread) Table 2 (c) Circumferential 25.5 20 137 × 180 direction(elongation) (d) Axial direction 44.4 Speed described in 184 × 100(spread) Table 2

[0037] The low-rate plastic working for elongation was conducted by ahydraulic press method, and the high-rate plastic working for spreadingwas conducted by a hammer press method. During the above plastic workingsteps, the temperature of the raw material was maintained at about 300°C. by the spontaneous heat.

Measurement of Average Crystal Grain Size

[0038] After polishing the surface of the obtained target material bysandpaper, the target material was etched with boiling nitric acid andthen subjected to electrolytic polishing to finish the surface of thetarget material into a mirror surface. Thereafter, the surface of thetarget material was etched with boiling nitric acid to expose a grainboundary thereof. The exposed grain boundary was magnified 800 times byan optical microscope and photographed. From the obtained photograph,the average crystal grain size was measured by a quadrature method. Theresults are shown in Table 2. TABLE 2 Examples and Processing AverageCrystal Number Comparative Rate Grain Size of Examples (%/second) (μm)“Particles” Comparative 10 70.0 72 Example 1 Comparative 20 39.4 60Example 2 Comparative 45 18.0 47 Example 3 Comparative 66 9.7 36 Example4 Comparative 88 5.2 8 Example 5 Example 1 100 3.4 2 Example 2 500 2.5 2Example 3 1,000 2.0 1 Example 4 2,000 1.8 1 Example 5 4,000 1.6 1Example 6 6,000 1.4 1

Determination of the Particles

[0039] The target material was cut into a disc having a diameter of 250mm and a thickness of 12 mm. The disc was placed in a sputtering deviceand sputtered under the following conditions: Power=3 kW; Gaspressure=10 mTorr; Gas ratio (Ar/N2)={fraction (1/1)}; and Filmthickness=50 nm. The sputtering formed a TiN film on a 6-inch siliconwafer. After completion of the sputtering, the number of “particles” inthe thin film formed on the silicon wafer was measured using alaser-type particle counter (trade name: “SF-6420”manufactured by TENCORInstruments Corp.). The number of “particles” having a diameter of atleast 3 μm was measured with respect to 12 silicon wafers, and theaverage of the measured values was determined to be the number of“particles” per one silicon wafer.

Aluminum Processing Examples Examples 7-12 and Comparative Examples 6-10(Shown in Table 4)

[0040] A round rod-shaped aluminum-alloy ingot composed of aluminum (apurity of 99.999% by weight) with 0.5% by weight copper is used as astarting material. The ingot had a diameter of 150 mm and a length of150 mm. The ingot was subjected to the plastic working steps (a) to (f)that are described below in Table 3. The plastic working steps werecontinuously conducted three times. Subsequent to the plastic working ofsteps (a) to (f), a further plastic working for spreading the rawmaterial (forging) was conducted at a processing rate of 20%/second,thereby forming the raw material into an appropriate shape and obtaininga target material having a size of 410 mm in diameter ×20 mm in length.TABLE 3 Pressure- applying Processing Processing Final Dimensiondirection Percentage Rate (diameter mm × (phenomenon) (%) (%/sec.)length) (a) Circumferential 8.7 20 137 × 180 direction (elongation) (b)Axial direction 44.4 Speed described 184 × 100 (spread) in Table 2 (c)Circumferential 25.5 20 137 × 180 direction (elongation) (d) Axialdirection 44.4 Speed described 184 × 100 (spread) in Table 2 (e)Circumferential 25.5 20 137 × 180 direction (elongation) (f) Axialdirection 44.4 Speed described 184 × 100 (spread) in Table 2

[0041] The low-rate plastic working for elongation was conducted using ahydraulic press, and the high-rate plastic working for spreading wasconducted using a hammer press. During the plastic working steps, thetemperature of the raw material was maintained in the range of from 50°C. to 450° C. For instance, the processing of Example 9 of Table 4(processing speed of 1,000%/second), was conducted as follows: Thetemperatures immediately before and immediately after the working step(b) were maintained at 30° C. and 100° C., respectively; thetemperatures immediately before the working step (d) (controlled bycooling) and that immediately after the working step (d) were maintainedat 80° C. and 150° C., respectively; and the temperatures immediatelybefore the working step (f) (controlled by cooling) and that immediatelyafter the working step (f) were maintained at 80° C. and 150° C.,respectively.

Measurement of Average Crystal Grain Size

[0042] After polishing the surface of the obtained target material by asandpaper, the target material was etched with an etching solutioncomposed of HCl:HNO3:HF:H2O=3:1:1:20 (weight ratio) to expose a grainboundary thereof. The exposed grain boundary was magnified 800 times byan optical microscope and photographed. From the obtained photograph,the average crystal grain size was measured by a quadrature method. Theresults are shown in Table 4.

Determination of the Particles

[0043] The target material was cut into a disc having a diameter of 250mm and a thickness of 12 mm. The disc was placed in a sputtering deviceand sputtered under the following conditions: Power=5 kW; Gas pressure=3mTorr; Sputtering gas=Ar (100%); and Film thickness=50 nm. Thesputtering formed an Al—Cu alloy film (0.5%, by weight, Cu) on a 6-inchsilicon wafer. After completion of the sputtering, the number of“particles” in the thin film formed on the silicon wafer was measuredusing a laser-type particle counter (SF-6420™ manufactured by TENCORInstruments Corp.). The number of “particles” having a diameter of atleast 0.2 μm was measured with respect to 12 silicon wafers, and theaverage of the measured values was determined to be the number of“particles” per one silicon wafer. TABLE 4 Examples and ProcessingAverage Crystal Number Comparative Rate Grain Size of Examples (%/sec.)(μm) “Particles” Comparative 10 200 82.3 Example 6 Comparative 13 15065.5 Example 7 Comparative 20 100 47.5 Example 8 Comparative 27 57 33.4Example 9 Comparative 52 30 20.9 Example 10 Example 7 100 20 5.6 Example8 500 10 3.9 Example 9 1,000 8 3.2 Example 10 2,000 6 2.7 Example 114,000 4 1.5 Example 12 6,000 2 1.3

[0044] The invention described herein can provide an industrially usefulprocess for producing target materials which are reduced in the numberof “particles” generated during a film-forming process relative toconventionally-produced target materials. In particular embodiments ofthe invention, the target materials can comprise one or more ofaluminum, titanium and copper. The invention can enable high throughputof materials by reducing processing steps. Specifically, a grain size ofa target material can be reduced simultaneously with the shaping of thematerial into a target shape by utilizing a die that is appropriatelyconfigured to form a target shape during high-rate plastic working. Theinvention can also reduce material waste since a processed material canbe formed into the shape of a target, and accordingly cutting and othermaterial removing steps can be avoided in forming targets.

[0045] In compliance with the statute, the invention has been describedin language more or less specific as to structural and methodicalfeatures. It is to be understood, however, that the invention is notlimited to the specific features shown and described, since the meansherein disclosed comprise preferred forms of putting the invention intoeffect. The invention is, therefore, claimed in any of its forms ormodifications within the proper scope of the appended claimsappropriately interpreted in accordance with the doctrine ofequivalents.

1. A method for reducing the grain size of a material, comprising:subjecting the material to plastic working at a processing rate of atleast 100%/second.
 2. The method of claim 1 further comprising shapingthe material into a sputtering target.
 3. The method of claim 2 whereinthe shaping occurs during the plastic working.
 4. The method of claim 1wherein the plastic working further comprises a processing percentage ofat least 5% while maintaining the processing rate of at least100%/second.
 5. The method of claim 1 wherein the material comprises oneor more of aluminum, copper and titanium.
 6. The method of claim 1wherein the material comprises aluminum, and further comprises at leastone element selected from the group consisting of Si, Cu, Ti, Cr, Mn,Zr, Hf and rare earth elements.
 7. The method of claim 1 wherein thematerial has an average grain size after the plastic working of lessthan 4 μm.
 8. The method of claim 1 wherein the processing rate is atleast 500%/second.
 9. The method of claim 1 wherein the processing rateis at least 1,000%/second.
 10. The method of claim 1 wherein theprocessing rate is at least 1,000%/second, and further comprising aprocessing percentage of at least 5% while maintaining the processingrate of at least 100%/second.
 11. The method of claim 1 wherein theprocessing rate is at least 2,000%/second.
 12. The method of claim 1wherein the processing rate is at least 4,000%/second.
 13. The method ofclaim 1 wherein the processing rate is at least 5,000%/second.
 14. Amethod for producing a sputtering target material, comprising:subjecting a titanium-comprising material to plastic working at aprocessing percentage of at least 5% utilizing a processing rate of atleast 100%/second.
 15. The method of claim 14 wherein thetitanium-comprising material is shaped into a sputtering target shapeduring the plastic working.
 16. The method of claim 14 wherein theplastic working is repeated a plurality of times.
 17. The method ofclaim 16 wherein said titanium-comprising material is maintained at atemperature of less than or equal to 400° C. during the plastic working.18. The method of claim 17 wherein the sputtering target material hastitanium grains; an average crystal grain size of the titanium grainsbeing not more than 4 μm.
 19. The method of claim 14 wherein saidtitanium-comprising material is maintained at a temperature of not morethan 400° C. during the plastic working.
 20. The method of claim 19wherein the sputtering target material has titanium grains; an averagecrystal grain size of the titanium grains being not more than 4 μm. 21.The method of claim 14 wherein the titanium-comprising material is atleast 99.99% pure in titanium.
 22. The method of claim 14 wherein thetitanium-comprising material is at least 99.9999% pure in titanium. 23.The method of claim 14 wherein the sputtering target material hastitanium grains; an average crystal grain size of the titanium grainsbeing not more than 4 μm.
 24. The method of claim 14 wherein theprocessing rate is at least 1,000%/second.
 25. The method of claim 14wherein the processing rate is at least 2,000%/second.
 26. The method ofclaim 14 wherein the processing rate is at least 4,000%/second.
 27. Themethod of claim 14 wherein the processing rate is at least5,000%/second.
 28. The method of claim 14 wherein the processing rate isat least 6,000%/second.
 29. A method for producing a sputtering targetmaterial, comprising: subjecting an aluminum-comprising material toplastic working at a processing percentage of at least 5% utilizing aprocessing rate of at least 100%/second.
 30. The method of claim 29wherein the aluminum-comprising material is shaped into a sputteringtarget shape during the plastic working.
 31. The method of claim 29wherein the plastic working is repeated a plurality of times.
 32. Themethod of claim 31 wherein said aluminum-comprising material ismaintained at a temperature of not more than 450° C. during the plasticworking.
 33. The method of claim 32 wherein the sputtering targetmaterial has aluminum grains; an average crystal grain size of thealuminum grains being not more than 20 μm.
 34. The method of claim 29wherein said aluminum-comprising material is maintained at a temperatureof not more than 450° C. during the plastic working.
 35. The method ofclaim 34 wherein the sputtering target material has aluminum grains; anaverage crystal grain size of the aluminum grains being not more than 20μm.
 36. The method of claim 34 wherein the sputtering target materialhas aluminum grains; an average crystal grain size of the aluminumgrains being not more than 10 μm.
 37. The method of claim 34 wherein thesputtering target material has aluminum grains; an average crystal grainsize of the aluminum grains being not more than 4 μm.
 38. The method ofclaim 34 wherein the sputtering target material has aluminum grains; anaverage crystal grain size of the aluminum grains being not more than 2μm.
 39. The method of claim 29 wherein the aluminum-comprising materialis at least 99.99% pure in aluminum.
 40. The method of claim 29 whereinthe aluminum-comprising material is at least 99.9999% pure in aluminum.41. The method of claim 29 wherein the aluminum-comprising materialcomprises at least one element selected from the group consisting of Si,Cu, Ti, Cr, Mn, Zr, Hf and rare earth elements.
 42. The method of claim29 wherein the sputtering target material has aluminum grains; anaverage crystal grain size of the aluminum grains being not more than 20μm.
 43. The method of claim 29 wherein the sputtering target materialhas aluminum grains; an average crystal grain size of the aluminumgrains being not more than 10 μm.
 44. The method of claim 29 wherein thesputtering target material has aluminum grains; an average crystal grainsize of the aluminum grains being not more than 4 μm.
 45. The method ofclaim 29 wherein the sputtering target material has aluminum grains; anaverage crystal grain size of the aluminum grains being not more than 2μm.
 46. The method of claim 29 wherein the processing rate is at least1,000%/second.
 47. The method of claim 29 wherein the processing rate isat least 2,000%/second.
 48. The method of claim 29 wherein theprocessing rate is at least 4,000%/second.
 49. The method of claim 29wherein the processing rate is at least 5,000%/second.
 50. The method ofclaim 29 wherein the processing rate is at least 6,000%/second.
 51. Amethod for producing a sputtering target material, comprising:subjecting a copper-comprising material to plastic working at aprocessing percentage of at least 5% utilizing a processing rate of atleast 100%/second.
 52. The method of claim 51 wherein thecopper-comprising material is shaped into a sputtering target shapeduring the plastic working.
 53. The method of claim 51 wherein theplastic working is repeated a plurality of times.
 54. The method ofclaim 51 wherein the copper-comprising material is at least 99.99% purein copper.
 55. The method of claim 51 wherein the copper-comprisingmaterial is at least 99.9999% pure in copper.
 56. The method of claim 51wherein the processing rate is at least 1,000%/second.
 57. The method ofclaim 51 wherein the processing rate is at least 2,000%/second.
 58. Themethod of claim 51 wherein the processing rate is at least4,000%/second.
 59. The method of claim 51 wherein the processing rate isat least 5,000%/second.
 60. The method of claim 51 wherein theprocessing rate is at least 6,000%/second.
 61. A material comprisingaluminum grains, with an average crystal grain size of the aluminumgrains being not more than 20 μm.
 62. The material of claim 61 being inthe shape of a sputtering target.
 63. The material of claim 61 being atleast 99.9999% pure in aluminum.
 64. The material of claim 61 comprisingat least one element selected from the group consisting of Si, Cu, Ti,Cr, Mn, Zr, Hf and rare earth elements.
 65. The material of claim 61wherein the average crystal grain size of the aluminum grains is notmore than 10 μm.
 66. The material of claim 61 wherein the averagecrystal grain size of the aluminum grains is not more than 4 μm.
 67. Thematerial of claim 61 wherein the average crystal grain size of thealuminum grains is not more than 2 μm.
 68. A material comprisingtitanium grains, with an average crystal grain size of the titaniumgrains being not more than 4 μm.
 69. The material of claim 68 whereinthe average crystal grain size of the titanium grains is not more than 2μm.
 70. The material of claim 68 being in the shape of a sputteringtarget.
 71. The material of claim 68 being at least 99.99% pure intitanium.
 72. The material of claim 68 being at least 99.9999% pure intitanium.